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Preparation method of anhydrous ceric sulfate

Anhydrous sulfuric acid and high cerium technology, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problem of poor water solubility of products, failure to meet the quality requirements of anhydrous ceric sulfate products, water insoluble advanced questions

Inactive Publication Date: 2010-01-27
甘肃稀土新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, this process is very dangerous to operate, and there are also requirements on equipment. From the perspective of environmental protection, pollution and corrosion are serious, and the possibility of industrial expansion is small.
Moreover, the product quality is poor in water solubility and high in water insoluble matter, which cannot meet the customer's requirements for the quality of anhydrous ceric sulfate products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Weigh 143 kg Ce(OH) 4 . Add 370 liters of deionized water to the enamel stirring tank, start stirring, slowly add 130 liters of industrial concentrated sulfuric acid and mix well, then slowly add the weighed cerium hydroxide into the acid solution, control the temperature to dissolve at 76°C, and dissolve for 40 minutes , heating up and concentrating, the crystallization temperature is 98°C, and the concentration time is 15 minutes. After cooling, the crystallized ceric sulfate is obtained by filtering, and the crystallized ceric sulfate is put into a crucible and put into a low-temperature resistance furnace for dehydration and drying. The temperature is 220°C, and the cerium oxide is measured as TREO. When ≥51%, it is released from the oven to obtain an orange-red powdery anhydrous ceric sulfate product. The product is water-soluble and can be dissolved and cleared within 25 minutes at room temperature. Its water solubility testing method is as follows: Weigh 5.3 gr...

Embodiment 2

[0013] Weigh 285 kg Ce(OH) 4 . Add 740 liters of deionized water into the enamel stirring tank, start stirring, slowly add 260 liters of industrial concentrated sulfuric acid and mix well, then slowly add the weighed cerium hydroxide into the acid solution, control the temperature to dissolve at 78°C, and dissolve for 35 minutes , heating up and concentrating, the crystallization temperature is 98°C, and the concentration time is 18 minutes. After cooling, the crystallized ceric sulfate is obtained by filtering, and the crystallized ceric sulfate is put into a crucible and put into a low-temperature resistance furnace for dehydration and drying. The temperature is 250°C, and the cerium oxide is measured as TREO. When ≥51%, it is released from the oven to obtain an orange-red powdery anhydrous ceric sulfate product. The product is water-soluble and dissolves clear within 20 minutes at room temperature. Product quality: CE 4+ / ∑Ce≥96%, CeO 2 / TREO≥99.90%, CL - ≤100PPm, PbO≤...

Embodiment 3

[0015] Weigh 429 kg Ce(OH) 4 . Add 1110 liters of deionized water into the enamel stirring tank, start stirring, slowly add 390 liters of industrial concentrated sulfuric acid and mix well, then slowly add the weighed cerium hydroxide into the acid solution, control the temperature to dissolve at 80°C, and dissolve for 50 minutes , heating up and concentrating, the crystallization temperature is 98°C, and the concentration time is 13 minutes. After cooling, it is filtered to obtain crystallized cerium sulfate. Put the crystallized cerium sulfate into a crucible and enter it into a low-temperature resistance furnace for dehydration and drying. The temperature is 230°C, and the cerium oxide is measured as TREO. When ≥51%, it is released from the oven to obtain an orange-red powdery anhydrous ceric sulfate product. The product is water-soluble and can be dissolved and cleared within 30 minutes at room temperature. Product quality: CE 4+ / ∑Ce≥96%, CeO 2 / TREO≥99.90%, CL - ≤10...

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Abstract

The invention discloses a preparation method of anhydrous ceric sulfate, taking high-purity cerium hydroxide as a raw material, and comprising the following steps: using industrial concentrated sulfuric acid to carry out acid dissolution on cerium hydroxide, controlling the (H<+>) mol / L of spent acid of the acid solution, the Ce<4+> dissolved concentration (g / L) of the acid solution and the dissolving temperature to fully dissolve the cerium hydroxide, then carrying out concentrated crystallization, cooling and filtering to obtain crystallized ceric sulfate which is put into a crucible and dehydrated and dried in a drying box, and then obtaining the product, namely anhydrous ceric sulfate. The anhydrous ceric sulfate prepared by the method has high product purity, good water solubility, short process flow and convenient operation, and is easy for scale production; in addition, the mother liquor can be reused, thereby playing a role of energy saving and emission elimination.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth sulfates, and in particular relates to a preparation method of anhydrous ceric sulfate. Background technique [0002] The traditional process of preparing anhydrous ceric sulfate: take cerium oxide with a purity of more than 99.9% and burn it at 800°C into a handle evaporating dish, add concentrated sulfuric acid, and heat it on the electric furnace until the particles are thin and thick and turn orange. Add pure water while hot to leach cerium sulfate, and go through two calcinations, take out and turn the material once in the middle, and prepare anhydrous ceric sulfate. Moreover, this process is very dangerous to operate, and there are also requirements on equipment. From the perspective of environmental protection, pollution and corrosion are serious, and the possibility of industrial expansion is small. Moreover, the product quality has poor water solubility and high water i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 于化琴李月红方中心周丽芳
Owner 甘肃稀土新材料股份有限公司
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